以提高激光诱导击穿光谱(LIBS)检测奶粉中重金属Cr元素精确性为研究目的,采用集成ICCD光谱仪的LIBS系统对奶粉样品中等离子体信号进行采集。为了减小检测误差,首先用洛伦兹(Lorentz)拟合对光谱谱线轮廓进行预处理,提取光谱净强度值。在...以提高激光诱导击穿光谱(LIBS)检测奶粉中重金属Cr元素精确性为研究目的,采用集成ICCD光谱仪的LIBS系统对奶粉样品中等离子体信号进行采集。为了减小检测误差,首先用洛伦兹(Lorentz)拟合对光谱谱线轮廓进行预处理,提取光谱净强度值。在相同的试验条件下,以Cr I 425.43 nm作为分析线、Ca I 422.67 nm作为内标线,分别采用外标法和内标法对奶粉中的Cr元素进行了定量分析,两种定标曲线的线性系数分别为0.946 52和0.991。实验结果表明,选取奶粉中基体元素Ca作为内标物质能有效提高定标曲线的拟合效果,减少误差,为将来采用内标法建模应用于便携式LIBS技术检测食品提供了参考。展开更多
Reduction of Cr(VI)using zero-valent iron(ZVI)could not only decrease the amounts of chemicals used for reduction,but also decrease the discharge of sludge.In order to find a desirable ZVI material,reduction of Cr(VI)...Reduction of Cr(VI)using zero-valent iron(ZVI)could not only decrease the amounts of chemicals used for reduction,but also decrease the discharge of sludge.In order to find a desirable ZVI material,reduction of Cr(VI)with a relative high concentration using different kinds of ZVI powders(mainly carbon differences)including reduced Fe,grey cast iron,pig iron,nodular pig iron was carried out.Parameters such as ZVI dosage,type and size affecting on Cr(VI)reduction were firstly examined and grey cast iron was selected as a preferable reducing material,followed by pig iron.Additionally,it was found that the parameters had significant influences on experimental kinetics.Then,morphology and composition of the sample before and after reaction were characterized by SEM,EPMA and XPS analyses to disclose carbon effect on the reducibility.In order to further interpret reaction mechanism,different reaction models were constructed.It was revealed that not only the carbon content could affect the Cr(VI)reduction,but also the carbon structure had an important effect on its reduction.展开更多
The variation of microstucture and phase structure of metal Cr and Al powders prepared by high energy mechanical milling was analyzed and investigated.The results show that with the continuous balling the average grai...The variation of microstucture and phase structure of metal Cr and Al powders prepared by high energy mechanical milling was analyzed and investigated.The results show that with the continuous balling the average grain sizes of the brittle Cr powders are gradually decreased,and the diffraction peaks are widened and the peak values lower owing to the interrelation caused by both cold welding and breaking;the tough Al powders exhibit intense cold welding,and most of powders lead to adhesion to ball surface and pot wall,meanwhile,the Al powders subjected to intense deformation have led to many dislocation rings with non dislocation wind up found in the microstructure.展开更多
At present, heavy metal pollution in food occurs frequently, which requires a novel method for rapid detection. Laser induced breakdown spectroscopy （LIBS） is a new technique for rapid and environmental friendly det...At present, heavy metal pollution in food occurs frequently, which requires a novel method for rapid detection. Laser induced breakdown spectroscopy （LIBS） is a new technique for rapid and environmental friendly detection, but it lacks high sensitivity and stability which restrict its development. In this study, Cr-polluted infant milk powder was used as experimental material to explore the feasibility of the application of LIBS technique in food safety detection. Aiming at improving the precision and accuracy of Cr detection by LIBS technique, LIBS spectra of samples were collected by a spectrometer with an intensified charge-cou- pled device （ICCD） using three gratings with different resolutions to comprehensively compare and analyze the stability, sensitivity and quantitative analysis accura- cy of LIBS detection. The results showed that average relative standard deviation （RSD） of LIBS spectral intensity was below 10%, indicating good stability. LIBS signals were collected by three gratings for quantitative analysis, and the results demonstrated that the linear correlation coefficient R2 of fitting curves was 0. 248 87, 0.903 12 and 0.992 81, respectively; the relative errors between actual and predicted concentrations were 38.23%, 8.84% and 7.43%, respectively, indicating that gratings with higher resolutions could lead to higher linear correlation coefficient and better detection accuracy. According to the results, high-resolu- tion spectrometer could significantly improve the accuracy of LIBS detection of Cr concentration in milk powder, suggesting that it is feasible to detect heavy metals in food by LIBS technique with the improvement of core device performance.展开更多
文摘以提高激光诱导击穿光谱(LIBS)检测奶粉中重金属Cr元素精确性为研究目的,采用集成ICCD光谱仪的LIBS系统对奶粉样品中等离子体信号进行采集。为了减小检测误差,首先用洛伦兹(Lorentz)拟合对光谱谱线轮廓进行预处理,提取光谱净强度值。在相同的试验条件下,以Cr I 425.43 nm作为分析线、Ca I 422.67 nm作为内标线,分别采用外标法和内标法对奶粉中的Cr元素进行了定量分析,两种定标曲线的线性系数分别为0.946 52和0.991。实验结果表明,选取奶粉中基体元素Ca作为内标物质能有效提高定标曲线的拟合效果,减少误差,为将来采用内标法建模应用于便携式LIBS技术检测食品提供了参考。
基金Project(51604131)supported by the National Natural Science Foundation of ChinaProject(2017FB084)supported by the Yunnan Province Applied Basic Research,China+1 种基金Project(KKSY201563041)supported by the Talent&Training Program of Yunnan Province,ChinaProjects(2017T20090159,2018T20150055)supported by the Testing and Analyzing Funds of Kunming University of Science and Technology,China
文摘Reduction of Cr(VI)using zero-valent iron(ZVI)could not only decrease the amounts of chemicals used for reduction,but also decrease the discharge of sludge.In order to find a desirable ZVI material,reduction of Cr(VI)with a relative high concentration using different kinds of ZVI powders(mainly carbon differences)including reduced Fe,grey cast iron,pig iron,nodular pig iron was carried out.Parameters such as ZVI dosage,type and size affecting on Cr(VI)reduction were firstly examined and grey cast iron was selected as a preferable reducing material,followed by pig iron.Additionally,it was found that the parameters had significant influences on experimental kinetics.Then,morphology and composition of the sample before and after reaction were characterized by SEM,EPMA and XPS analyses to disclose carbon effect on the reducibility.In order to further interpret reaction mechanism,different reaction models were constructed.It was revealed that not only the carbon content could affect the Cr(VI)reduction,but also the carbon structure had an important effect on its reduction.
文摘The variation of microstucture and phase structure of metal Cr and Al powders prepared by high energy mechanical milling was analyzed and investigated.The results show that with the continuous balling the average grain sizes of the brittle Cr powders are gradually decreased,and the diffraction peaks are widened and the peak values lower owing to the interrelation caused by both cold welding and breaking;the tough Al powders exhibit intense cold welding,and most of powders lead to adhesion to ball surface and pot wall,meanwhile,the Al powders subjected to intense deformation have led to many dislocation rings with non dislocation wind up found in the microstructure.
文摘At present, heavy metal pollution in food occurs frequently, which requires a novel method for rapid detection. Laser induced breakdown spectroscopy （LIBS） is a new technique for rapid and environmental friendly detection, but it lacks high sensitivity and stability which restrict its development. In this study, Cr-polluted infant milk powder was used as experimental material to explore the feasibility of the application of LIBS technique in food safety detection. Aiming at improving the precision and accuracy of Cr detection by LIBS technique, LIBS spectra of samples were collected by a spectrometer with an intensified charge-cou- pled device （ICCD） using three gratings with different resolutions to comprehensively compare and analyze the stability, sensitivity and quantitative analysis accura- cy of LIBS detection. The results showed that average relative standard deviation （RSD） of LIBS spectral intensity was below 10%, indicating good stability. LIBS signals were collected by three gratings for quantitative analysis, and the results demonstrated that the linear correlation coefficient R2 of fitting curves was 0. 248 87, 0.903 12 and 0.992 81, respectively; the relative errors between actual and predicted concentrations were 38.23%, 8.84% and 7.43%, respectively, indicating that gratings with higher resolutions could lead to higher linear correlation coefficient and better detection accuracy. According to the results, high-resolu- tion spectrometer could significantly improve the accuracy of LIBS detection of Cr concentration in milk powder, suggesting that it is feasible to detect heavy metals in food by LIBS technique with the improvement of core device performance.
